HuagongsheHuagongshe Chemistry Print Report · For research reference only
Tributylamine → Isobutyl 2-hydroxy-5-[2-[4-[(3-methyl-2-pyridinylamino)sulfonyl]phenyl]ethenyl]benzoate
Participants
| Role | Name | HCID | Charge |
|---|---|---|---|
| Reactant | Tributylamine | HCID 7622 | — |
| Reactant | HCID 3792615 | HCID 3792615 | — |
| Reactant | Isobutyl 5-ethenyl-2-hydroxybenzoate | HCID 19423382 | — |
| Catalyst | Palladium | HCID 23938 | — |
| Solvent | Dimethylacetamide | HCID 31374 | — |
| Product | Isobutyl 2-hydroxy-5-[2-[4-[(3-methyl-2-pyridinylamino)sulfonyl]phenyl]ethenyl]benzoate | HCID 54356729 | 51.4% |
Reaction Steps
10% Palladium on charcoal (0.5g) was added to a solution of isobutyl 5-ethenyl-2-hydroxybenzoate (6.6 g, 30mmol) and 4-iodo-N-(3-methyl-2-pyridinyl)benzenesulfonamide (11.2 g, 30 mmol) in dimethylacetamide (10 ml) and tributylamine (10 ml, 42 mmol) at 110° C. After 90 min. the solution was filtered and diluted with isopropanol (0.3 l) and chilled in a freezer. The product was filtered off, dried and dissolved in boiling formic acid (100 ml). The solution was filtered and water (65 ml) was added. After cooling to refrigerator temperature the product was filtered off and dried to yield 7.2 g (51%) product
Provenance & Evidence
| DOI | 10.6084/m9.figshare.5104873.v1 |
|---|---|
| Patent number | US05302718 |
| Source dataset | uspto-grants-1994_04 |
| ORD ID | ord-87e8454b11784379b44bdfe542a751f5 |
| Source note | uspto-grants-1994_04 |